CN112071944B - Ultraviolet photodiode based on NiFe2O4/Ga2O3 and preparation method thereof - Google Patents
Ultraviolet photodiode based on NiFe2O4/Ga2O3 and preparation method thereof Download PDFInfo
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- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910003264 NiFe2O4 Inorganic materials 0.000 title claims abstract description 77
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 15
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims abstract description 77
- 239000000758 substrate Substances 0.000 claims abstract description 62
- 238000004140 cleaning Methods 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000004544 sputter deposition Methods 0.000 claims description 187
- 238000004528 spin coating Methods 0.000 claims description 77
- 238000010438 heat treatment Methods 0.000 claims description 60
- 238000000137 annealing Methods 0.000 claims description 57
- 239000013077 target material Substances 0.000 claims description 50
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 40
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 34
- 238000005477 sputtering target Methods 0.000 claims description 29
- 238000000151 deposition Methods 0.000 claims description 24
- 230000008021 deposition Effects 0.000 claims description 24
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 20
- 229910009112 xH2O Inorganic materials 0.000 claims description 20
- 239000003381 stabilizer Substances 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 229910010293 ceramic material Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000003980 solgel method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000007769 metal material Substances 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 229910002370 SrTiO3 Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000009987 spinning Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 28
- 238000001514 detection method Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 229910001195 gallium oxide Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
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Abstract
The invention discloses a method based on NiFe2O4/Ga2O3The invention also discloses an ultraviolet photodiode based on NiFe2O4/Ga2O3Firstly, cleaning a substrate, and drying the substrate by using nitrogen for later use; carrying out P-type NiFe on the cleaned substrate2O4Growing a layer; in the obtained P-type NiFe2O4Carrying out N-type beta-Ga on partial region on the layer2O3Growing a layer; in the obtained P-type NiFe2O4Fabricating P-type NiFe on the layer2O4An electrode on the layer; in the obtained N-type beta-Ga2O3Fabricating N-type beta-Ga layer on top of layer2O3Electrodes on the layers to ultimately form the NiFe-based2O4/Ga2O3The ultraviolet photodiode of (1). The invention solves the problem that in the prior art, p-type Ga2O3Lack of material and inability to produce Ga2O3A pn junction-based ultraviolet photodiode.
Description
Technical Field
The invention belongs to the technical field of ultraviolet photoelectric detection application, and particularly relates to a NiFe-based photoelectric detection device2O4/Ga2O3The invention also relates to a NiFe-based ultraviolet photodiode2O4/Ga2O3The method of manufacturing an ultraviolet photodiode of (1).
Background
Gallium oxide (. beta. -Ga)2O3) As a novel direct band gap wide band gap semiconductor material, the band gap width is 4.9eV, the corresponding absorption wavelength is 253nm, the photoelectric response characteristic is high in a deep ultraviolet region, and the direct band gap wide band gap semiconductor material has great application potential in the field of deep ultraviolet solar blind photodetectors. At the same time, the content of gallium oxide is highThe breakdown electric field intensity with high forbidden band width (the theoretical value of the critical breakdown electric field intensity can reach 8MV/cm) enables the gallium oxide deep ultraviolet solar blind photoelectric detector to be more suitable for application in high-frequency, high-temperature, high-voltage and high-radiation environments.
At present, Ga2O3The ultraviolet photodetector is mainly based on a schottky (MSM) structure. Compared with the photodetector based on the MSM structure, the photodetector based on the pn junction structure has a larger photoresponse and a faster corresponding speed. However, due to the presence of oxygen vacancies, p-type Ga is currently present2O3No effective progress has been made in the preparation of the materials. p type Ga2O3The absence of material causes Ga2O3The ultraviolet photodiode with base pn junction structure is difficult to realize, thereby restricting Ga2O3The material is applied to the field of ultraviolet photoelectric detection.
Disclosure of Invention
The invention aims to provide a method based on NiFe2O4/Ga2O3The ultraviolet photodiode solves the problem of p-type Ga in the prior art2O3Lack of material and inability to produce Ga2O3The pn junction-based ultraviolet photodiode.
Another object of the present invention is to provide a method for producing a NiFe-based alloy2O4/Ga2O3The method of manufacturing an ultraviolet photodiode of (1).
The first technical scheme adopted by the invention is based on NiFe2O4/Ga2O3The ultraviolet photodiode comprises a substrate, and P-type NiFe is formed on the substrate2O4Layer of P-type NiFe2O4N-type beta-Ga is formed on partial region of the layer2O3Layer of N-type beta-Ga2O3On the layer is N-type beta-Ga2O3Electrode on layer, P-type NiFe2O4P-type NiFe is formed on the other partial region of the layer2O4An electrode on the layer.
The first technical means of the present invention is also characterized in that,
p-type NiFe2O4Electrode on layer and N-type beta-Ga2O3The electrode material on the layer is one of Au, Al, Ni, Ti, Cu and Pb metal materials, or alloy containing the metal materials or ITO conductive compound.
The substrate is Al2O3Quartz, insulating MgO or insulating SrTiO3A substrate.
N-type beta-Ga2O3The layer thickness is 100-200 nm, the doping concentration is 1015～1016cm-3Said P type NiFe2O4The layer thickness is 100-200 nm, and the carrier concentration is 1017～1018cm-3。
The second technical scheme adopted by the invention is that the alloy is based on NiFe2O4/Ga2O3The preparation method of the ultraviolet photodiode is implemented according to the following steps:
step 4, obtaining the P type NiFe in the step 22O4Fabricating P-type NiFe on the layer2O4An electrode on the layer;
step 5, obtaining N-type beta-Ga in step 32O3Layer-by-layer fabrication of N-type beta-Ga2O3Electrodes on the layers to ultimately form the NiFe-based2O4/Ga2O3The ultraviolet photodiode of (1).
The second technical aspect of the present invention is also characterized in that,
the cleaning process in the step 1 comprises the following steps: the samples were washed step by step using a wash solution-acetone-alcohol-deionized water.
P-type NiFe on the substrate in step 22O4The layer is grown by adopting a magnetron sputtering device and NiFe2O4Ceramic material as target material, argon Ar and oxygen O2As a sputtering gas, Ar: O during sputtering2The proportion is 10: 1-5: 1, the substrate temperature is 500-600 ℃, the sputtering pressure is controlled to be 0.5-5 Pa, the sputtering power is controlled to be 100-200W, the sputtering time is controlled to be 0.1-5 hours, then a sample obtained by sputtering is annealed in an air environment, the annealing temperature is 600-700 ℃, the annealing time is 0.5-2 hours, and the P-type NiFe is obtained2O4A heteroepitaxial layer.
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute and glycol methyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As a stabilizer, the concentration of the solution is 0.3-0.6 mol/L;
step 3.2, stirring the solution obtained in the step 3.1 at a constant temperature of 60-70 ℃ for 2-3 hours to form sol, and filtering the sol after aging for 36-48 hours;
step 3.3, spin-coating the sol prepared in the step 3.2 on P-type NiFe2O4On the layer, the spin coating speed is controlled to be 2500-3000 rpm during spin coating, the spin coating time is controlled to be 30-45 seconds, the material obtained after spin coating is subjected to low-temperature heat treatment for 10-40 minutes in an air environment at the temperature of 100-200 ℃, and then is subjected to high-temperature heat treatment for 10-40 minutes at the temperature of 500-700 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the material is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the repetition times of the spin coating and the heat treatment to prepare the N-type beta-Ga2O3The thickness of the layer;
step 3.5, the spin coating and the heat treatment are finished to obtainThe obtained material is placed in an air environment for annealing treatment, the annealing temperature is 600-1000 ℃, the annealing time is 1-3 hours, and N-type beta-Ga is obtained2O3And (3) a layer.
P type NiFe in step 42O4When the electrode is manufactured on the layer, magnetron sputtering is adopted, and Ti is firstly used as a sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1-2 hours, the sputtering pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W; and then, sputtering Au as a sputtering target material on the surface of the Ti layer to form an Au layer, wherein the sputtering time is controlled to be 0.1-2 hours, the sputtering pressure is controlled to be 2-4 Pa, and the sputtering power is 10-20 mW.
In step 5 in N-type beta-Ga2O3When electrodes are manufactured on the layers, magnetron sputtering is adopted, firstly, Ni is used as a target material, the deposition time is controlled to be 0.1-2 hours, the deposition pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W; and then, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, wherein the deposition time is controlled to be 0.1-2 hours, the deposition pressure is controlled to be 2-4 Pa, the sputtering power is 10-20 mW, and finally the NiFe-based material is formed2O4/Ga2O3The ultraviolet photodiode of (1).
The invention has the beneficial effects that the alloy is based on NiFe2O4/Ga2O3The ultraviolet photodiode adopts NiFe with excellent optical performance for the first time2O4And Ga2O3Forming heterojunction and fully exerting Ga2O3The application potential of the material in the solar blind ultraviolet detection field; meanwhile, Ga is compared with SiC, GaN and the like2O3The material has larger forbidden band width and higher critical breakdown electric field intensity, so that the NiFe-based material of the invention2O4/Ga2O3The ultraviolet photodiode of (2) has a higher withstand voltage level. Under extreme conditions of high temperature, high pressure, high frequency and high radiation, the NiFe-based alloy of the invention2O4/Ga2O3The novel ultraviolet photoelectric detector of the ultraviolet photoelectric diode not only has better detection performance than the prior ultraviolet photoelectric detectorThe detector and the reliability of the device are greatly improved, so that the detector is more suitable for the extreme environment.
Drawings
FIG. 1 shows a NiFe-based alloy of the present invention2O4/Ga2O3The ultraviolet photodiode structure of (1);
FIG. 2 shows a NiFe-based alloy of the present invention2O4/Ga2O3The flow chart of the method for manufacturing an ultraviolet photodiode of (1).
In the figure, 1 is a substrate, 2 is a P-type NiFe2O4Layer, 3.P type NiFe2O4Electrode on layer, 4.N type beta-Ga2O3Layer, 5.N type beta-Ga2O3An electrode on the layer.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention is based on NiFe2O4/Ga2O3The ultraviolet photodiode of (1) is shown in figure 1, and comprises a substrate 1, wherein P-type NiFe is formed on the substrate 12O4Layer 2, P type NiFe2O4N-type beta-Ga is formed on a partial region of the layer 22O3Layer 4, N-type beta-Ga2O3On layer 4 is N-type beta-Ga2O3Electrode 5 on the layer, P-type NiFe2O4The other partial region of the layer 2 is formed with P-type NiFe2O4An electrode 3 on the layer.
P type NiFe2O4Electrode 3 on the layer and N-type beta-Ga2O3The electrode 5 on the layer is made of one of Au, Al, Ni, Ti, Cu and Pb metal materials, or alloy containing the metal materials or ITO conductive compound.
The substrate 1 is Al2O3Quartz, insulating MgO or insulating SrTiO3A substrate.
N-type beta-Ga2O3The layer 4 has a thickness of 100-200 nm and a doping concentration of 1015～1016cm-3Said P type NiFe2O4Layer 2 thicknessThe degree of the transition metal oxide is 100 to 200nm, and the carrier concentration is 1017～1018cm-3。
Based on NiFe2O4/Ga2O3The flow chart of the preparation method of the ultraviolet photodiode is shown in fig. 2, and the preparation method is implemented according to the following steps:
the cleaning process in the step 1 comprises the following steps: the samples were washed step by step using a wash solution-acetone-alcohol-deionized water.
p-type NiFe on substrate 1 in step 22O4The layer growth adopts magnetron sputtering equipment and NiFe2O4Ceramic material as target material, argon Ar and oxygen O2As a sputtering gas, Ar: O during sputtering2The proportion is 10: 1-5: 1, the substrate temperature is 500-600 ℃, the sputtering pressure is controlled to be 0.5-5 Pa, the sputtering power is controlled to be 100-200W, the sputtering time is controlled to be 0.1-5 hours, then a sample obtained by sputtering is annealed in an air environment, the annealing temperature is 600-700 ℃, the annealing time is 0.5-2 hours, and the P-type NiFe is obtained2O4A heteroepitaxial layer.
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute and glycol methyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As a stabilizer, the concentration of the solution is 0.3-0.6 mol/L;
step 3.2, stirring the solution obtained in the step 3.1 at a constant temperature of 60-70 ℃ for 2-3 hours to form sol, and filtering the sol after aging for 36-48 hours;
step 3.3, spin-coating the sol prepared in the step 3.2 on P-type NiFe2O4On the layer, the spin coating speed is controlled to be 2500-3000 rpm during spin coating, the spin coating time is controlled to be 30-45 seconds, the material obtained after spin coating is subjected to low-temperature heat treatment for 10-40 minutes in an air environment at the temperature of 100-200 ℃, and then is subjected to high-temperature heat treatment for 10-40 minutes at the temperature of 500-700 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the material is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the repetition times of the spin coating and the heat treatment to prepare the N-type beta-Ga2O3The thickness of the layer;
step 3.5, placing the material obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 600-1000 ℃, and the annealing time is 1-3 hours to obtain the N-type beta-Ga2O3And (3) a layer.
Step 4, obtaining the P type NiFe in the step 22O4Making P-type NiFe on the layer2O4An electrode 3 on the layer;
p type NiFe in step 42O4The electrode is made by magnetron sputtering, firstly Ti is used as sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1-2 hours, the sputtering pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W; and then, sputtering Au as a sputtering target material on the surface of the Ti layer to form an Au layer, wherein the sputtering time is controlled to be 0.1-2 hours, the sputtering pressure is controlled to be 2-4 Pa, and the sputtering power is 10-20 mW.
Step 5, obtaining N-type beta-Ga in step 32O3Fabricating N-type beta-Ga layer on top of layer2O3An electrode 5 on the layer eventually forming said NiFe-based2O4/Ga2O3Ultraviolet photoelectric deviceA pole tube.
In step 5 in N-type beta-Ga2O3When electrodes are manufactured on the layers, magnetron sputtering is adopted, firstly, Ni is used as a target material, the deposition time is controlled to be 0.1-2 hours, the deposition pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W; and then, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, wherein the deposition time is controlled to be 0.1-2 hours, the deposition pressure is controlled to be 2-4 Pa, the sputtering power is 10-20 mW, and finally the NiFe-based material is formed2O4/Ga2O3The ultraviolet photodiode of (1).
Example 1
Based on NiFe2O4/Ga2O3The flow chart of the preparation method of the ultraviolet photodiode is shown in fig. 2, and the preparation method is implemented according to the following steps:
the cleaning process in the step 1 comprises the following steps: the samples were washed step by step using a wash solution-acetone-alcohol-deionized water.
p-type NiFe on substrate 1 in step 22O4The layer growth adopts magnetron sputtering equipment and NiFe2O4Ceramic material as target material, argon Ar and oxygen O2As sputtering gas, Ar: O in sputtering2The proportion is 10:1, the substrate temperature is 500 ℃, the sputtering pressure is controlled to be 0.5Pa, the sputtering power is controlled to be 100W, the sputtering time is controlled to be 0.1 hour, then the sample obtained by sputtering is annealed in the air environment, the annealing temperature is 600 ℃, the annealing time is 0.5 hour, and the P-type NiFe is obtained2O4A heteroepitaxial layer.
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute, ethylene glycol monomethyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As a stabilizer, the concentration of the solution is 0.3 mol/L;
step 3.2, stirring the solution obtained in the step 3.1 at a constant temperature of 60 ℃ for 2 hours to form sol, and filtering the sol after aging for 36 hours;
step 3.3, spin-coating the sol prepared in the step 3.2 on P-type NiFe2O4On the layer, the spin-coating rotation speed is controlled to be 2500rpm during spin-coating, the rotation time is controlled to be 30 seconds, the material obtained after spin-coating is subjected to low-temperature heat treatment for 10 minutes in an air environment at 100 ℃, and then is subjected to high-temperature heat treatment for 10 minutes at 500 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the material is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the repetition times of the spin coating and the heat treatment to prepare the N-type beta-Ga2O3The thickness of the layer;
step 3.5, placing the material obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 600 ℃, and the annealing time is 1 hour to obtain the N-type beta-Ga2O3A layer.
Step 4, obtaining the P type NiFe in the step 22O4Making P-type NiFe on the layer2O4An electrode 3 on the layer;
p type NiFe in step 42O4The electrode is made by magnetron sputtering, firstly Ti is used as sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1 hour, the sputtering pressure is controlled to be 0.1Pa, and the sputtering power is controlled to be 100W; then Au is taken as a sputtering target material to be arranged on the surface of the Ti layerAnd sputtering to form an Au layer, wherein the sputtering time is controlled to be 0.1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Step 5, obtaining N-type beta-Ga in step 32O3Fabricating N-type beta-Ga layer on top of layer2O3Electrode 5 on the layer eventually forming said NiFe-based2O4/Ga2O3The ultraviolet photodiode of (1).
In step 5 in N-type beta-Ga2O3When electrodes are manufactured on the layers, magnetron sputtering is adopted, firstly Ni is used as a target material, the deposition time is controlled to be 0.1 hour, the deposition pressure is controlled to be 0.1Pa, and the sputtering power is controlled to be 100W; and then, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, wherein the deposition time is controlled to be 0.1 hour, the deposition pressure is controlled to be 2Pa, the sputtering power is 10mW, and finally the NiFe-based Ni layer is formed2O4/Ga2O3The ultraviolet photodiode of (1).
Example 2
Based on NiFe2O4/Ga2O3The flow chart of the preparation method of the ultraviolet photodiode is shown in fig. 2, and the preparation method is implemented according to the following steps:
the cleaning process in the step 1 comprises the following steps: the samples were washed step by step using a wash solution acetone-alcohol-deionized water.
p-type NiFe on substrate 1 in step 22O4The layer is grown by adopting a magnetron sputtering device and NiFe2O4Ceramic material as target material, argon Ar and oxygen O2As a sputtering gas, Ar: O during sputtering2The proportion is 5:1, the substrate temperature is 600 ℃, the sputtering pressure is controlled to be 5Pa, the sputtering power is controlled to be 200W, the sputtering time is controlled to be 5 hours, then the sample obtained by sputtering is annealed in the air environment, the annealing temperature is 700 ℃, the annealing time is 2 hours, and the P-type NiFe is obtained2O4A heteroepitaxial layer.
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute and glycol methyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As a stabilizer, the concentration of the solution is 0.6 mol/L;
step 3.2, stirring the solution obtained in the step 3.1 at the constant temperature of 60-70 ℃ for 3 hours to form sol, and filtering the sol after aging for 48 hours;
step 3.3, spin-coating the sol prepared in the step 3.2 on P-type NiFe2O4On the layer, the spin-coating rotating speed is controlled to be 3000rpm during spin-coating, the rotating time is 45 seconds, the material obtained after spin-coating is subjected to low-temperature heat treatment for 40 minutes in an air environment at the temperature of 200 ℃, and then the material is subjected to high-temperature heat treatment for 40 minutes at the temperature of 700 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the material is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the repetition times of the spin coating and the heat treatment to prepare the N-type beta-Ga2O3The thickness of the layer;
step 3.5, placing the material obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 1000 ℃, and the annealing time is 3 hours to obtain the N-type beta-Ga2O3A layer.
Step 4, obtaining the P type NiFe in the step 22O4Fabricating P-type NiFe on the layer2O4An electrode 3 on the layer;
p type NiFe in step 42O4When the electrode is manufactured on the layer, magnetron sputtering is adopted, and Ti is firstly used as a sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, controlling the sputtering time to be 2 hours, controlling the sputtering pressure to be 10Pa, and controlling the sputtering power to be 200W; and then, Au is taken as a sputtering target material to form an Au layer on the surface of the Ti layer by sputtering, the sputtering time is controlled to be 2 hours, the sputtering pressure is controlled to be 4Pa, and the sputtering power is 20 mW.
Step 5, obtaining N-type beta-Ga in step 32O3Layer-by-layer fabrication of N-type beta-Ga2O3An electrode 5 on the layer eventually forming said NiFe-based2O4/Ga2O3The ultraviolet photodiode of (1).
In step 5 in N-type beta-Ga2O3When electrodes are manufactured on the layers, magnetron sputtering is adopted, firstly Ni is used as a target material, the deposition time is controlled to be 2 hours, the deposition pressure is controlled to be 10Pa, and the sputtering power is controlled to be 200W; and then, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, wherein the deposition time is controlled to be 2 hours, the deposition pressure is controlled to be 4Pa, the sputtering power is 20mW, and finally the NiFe-based Ni layer is formed2O4/Ga2O3The ultraviolet photodiode of (1).
Example 3
Based on NiFe2O4/Ga2O3The flow chart of the preparation method of the ultraviolet photodiode is shown in fig. 2, and the preparation method is implemented according to the following steps:
the cleaning process in the step 1 comprises the following steps: the samples were washed step by step using a wash solution-acetone-alcohol-deionized water.
p-type NiFe on substrate 1 in step 22O4The layer is grown by adopting a magnetron sputtering device and NiFe2O4Ceramic material as target material, argon Ar and oxygen O2As a sputtering gas, sputteringAr is O at the time of injection2The proportion is 8:1, the substrate temperature is 550 ℃, the sputtering pressure is controlled to be 3Pa, the sputtering power is controlled to be 150W, the sputtering time is controlled to be 3 hours, then the sample obtained by sputtering is annealed in the air environment, the annealing temperature is 650 ℃, the annealing time is 1 hour, and the P-type NiFe is obtained2O4A heteroepitaxial layer.
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute and glycol methyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As a stabilizer, the concentration of the solution is 0.5 mol/L;
step 3.2, stirring the solution obtained in the step 3.1 at 65 ℃ for 2.5 hours to form sol, aging for 40 hours, and filtering the sol;
step 3.3, spin-coating the sol prepared in the step 3.2 on P-type NiFe2O4On the layer, the spin coating speed is controlled to be 2800rpm during spin coating, the spin coating time is 40 seconds, the material obtained after spin coating is subjected to low-temperature heat treatment for 20 minutes in an air environment at the temperature of 150 ℃, and then the material is subjected to high-temperature heat treatment for 30 minutes at the temperature of 600 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the material is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the repetition times of the spin coating and the heat treatment to prepare the N-type beta-Ga2O3The thickness of the layer;
step 3.5, placing the material obtained after the spin coating and the heat treatment in an air environmentAnnealing at 800 deg.C for 2 hr to obtain N-type beta-Ga2O3A layer.
Step 4, obtaining the P type NiFe in the step 22O4Making P-type NiFe on the layer2O4An electrode 3 on the layer;
p type NiFe in step 42O4When the electrode is manufactured on the layer, magnetron sputtering is adopted, and Ti is firstly used as a sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 150W; and then, Au is taken as a sputtering target material to form an Au layer on the surface of the Ti layer by sputtering, the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 3Pa, and the sputtering power is 15 mW.
Step 5, obtaining N-type beta-Ga in step 32O3Layer-by-layer fabrication of N-type beta-Ga2O3An electrode 5 on the layer eventually forming said NiFe-based2O4/Ga2O3The ultraviolet photodiode of (1).
In step 5 in N-type beta-Ga2O3Magnetron sputtering is adopted when the electrode is manufactured on the layer, firstly Ni is used as a target material, the deposition time is controlled to be 1 hour, the deposition pressure is controlled to be 5Pa, and the sputtering power is controlled to be 150W; and then, sputtering Au serving as a sputtering target material on the surface of the Ni layer to form an Au layer, wherein the deposition time is controlled to be 1 hour, the deposition pressure is controlled to be 3Pa, the sputtering power is 15mW, and finally the NiFe-based Ni layer is formed2O4/Ga2O3The ultraviolet photodiode of (1).
Example 4
The invention is based on NiFe2O4/Ga2O3As shown in fig. 2, the method for manufacturing an ultraviolet photodiode specifically includes the following steps:
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute, ethylene glycol monomethyl ether (CH)3OCH2CH2OH) as solvent, ethanolamine (HOCH)2CH2NH2) As a stabilizer, the concentration of the solution is 0.3 mol/L;
step 3.2, stirring the solution obtained in the step 1 at a constant temperature of 60 ℃ for two hours to form sol, aging for 36 hours, and filtering the sol;
3.3, spin-coating the sol prepared in the step 2 on an intrinsic SiC homogeneous epitaxial layer, controlling the spin-coating rotation speed to be 3000rpm during spin-coating, controlling the spin-coating rotation time to be 30 seconds, carrying out low-temperature heat treatment on a sample obtained after spin-coating for 40 minutes in an air environment at 100 ℃, and then carrying out high-temperature heat treatment for 10 minutes at 700 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the sample is cooled to the room temperature in the air, spin coating and heat treatment are carried out according to the step 3.3, and the repetition times of the spin coating and the heat treatment are adjusted to control the prepared N-type beta-Ga2O3The thickness of the layer is 110 nm;
and 3.5, placing the sample obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 800 ℃, and the annealing time is 2 hours.
Step 4, adopting a magnetron sputtering method to perform P-type NiFe2O4Making electrode on the layer, firstly using Ti as sputtering target material and making it be in P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is controlled to be 100W; and then, Au is taken as a sputtering target material to form an Au layer on the surface of the Ti layer by sputtering, the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Step 5, adopting a magnetron sputtering method to carry out magnetron sputtering on the N-type beta-Ga2O3Making electrodes on the layer, firstly using Ni as target material on N-type beta-Ga2O3Sputtering the surface of the layer to form a Ni layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 4 and controlling the sputtering power to be 100; and then, Au is taken as a sputtering target material to form an Au layer on the surface of the Ni layer by sputtering, the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Example 5
The invention relates to a method based on NiFe2O4/Ga2O3As shown in fig. 2, the method for manufacturing an ultraviolet photodiode is specifically implemented according to the following steps:
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute, ethylene glycol monomethyl ether (CH)3OCH2CH2OH) as solvent, ethanolamine (HOCH)2CH2NH2) As a stabilizer, the concentration of the solution is 0.3 mol/L;
step 3.2, stirring the solution obtained in the step 1 for two hours at a constant temperature of 60 ℃ to form sol, and filtering the sol after aging for 36 hours;
3.3, spin-coating the sol prepared in the step 2 on the intrinsic SiC homoepitaxial layer, controlling the spin-coating speed to 3000rpm during spin-coating and the spin-coating time to be 30 seconds, carrying out low-temperature heat treatment on a sample obtained after spin-coating for 40 minutes in an air environment at 100 ℃, and then carrying out high-temperature heat treatment for 10 minutes at 700 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the sample is cooled to the room temperature in the air, spin coating and heat treatment are carried out according to the step 3.3, and the repetition times of the spin coating and the heat treatment are adjusted to control the prepared N-type beta-Ga2O3The thickness of the layer is 110 nm;
and 3.5, placing the sample obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 800 ℃, and the annealing time is 2 hours.
Step 4, adopting a magnetron sputtering method to perform P-type NiFe2O4An electrode is made on the layer, Ti is firstly used as a sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 2Pa and controlling the sputtering power to be 100W; then sputtering AuAnd sputtering the target material on the surface of the Ti layer to form an Au layer, wherein the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Step 5, adopting a magnetron sputtering method to carry out magnetron sputtering on the N-type beta-Ga2O3Preparing electrodes on the layer, firstly using Ni as target material to make N-type beta-Ga2O3Sputtering the surface of the layer to form a Ni layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 4 and controlling the sputtering power to be 100; and then, Au is taken as a sputtering target material to form an Au layer on the surface of the Ni layer by sputtering, the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Example 6
The invention relates to a method based on NiFe2O4/Ga2O3As shown in fig. 2, the method for manufacturing an ultraviolet photodiode is specifically implemented according to the following steps:
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute, ethylene glycol monomethyl ether (CH)3OCH2CH2OH) as solvent, ethanolamine (HOCH)2CH2NH2) As a stabilizer, the concentration of the solution is 0.4 mol/L;
step 3.2, stirring the solution obtained in the step 1 at a constant temperature of 60 ℃ for two hours to form sol, aging for 36 hours, and filtering the sol;
3.3, spin-coating the sol prepared in the step 2 on the intrinsic SiC homoepitaxial layer, controlling the spin-coating speed to 3000rpm during spin-coating, controlling the spin-coating time to be 30 seconds, carrying out low-temperature heat treatment on a sample obtained after spin-coating at 150 ℃ in an air environment for 30 minutes, and then carrying out high-temperature heat treatment at 600 ℃ for 25 minutes by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the sample is cooled to the room temperature in the air, spin coating and heat treatment are carried out according to the step 3.3, and the repetition times of the spin coating and the heat treatment are adjusted to control the prepared N-type beta-Ga2O3The thickness of the layer is 150 nm;
and 3.5, placing the sample obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 800 ℃, and the annealing time is 2 hours.
Step 4, adopting a magnetron sputtering method to carry out P-type NiFe2O4An electrode is made on the layer, Ti is firstly used as a sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 2Pa and controlling the sputtering power to be 100W; and then, sputtering Au as a sputtering target material on the surface of the Ti layer to form an Au layer, wherein the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Step 5, adopting a magnetron sputtering method to carry out magnetron sputtering on the N-type beta-Ga2O3Preparing electrodes on the layer, firstly using Ni as target material to make N-type beta-Ga2O3Sputtering the surface of the layer to form a Ni layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 4 and controlling the sputtering power to be 100; then is provided withAnd Au is used as a sputtering target material to sputter on the surface of the Ni layer to form an Au layer, the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 2Pa, and the sputtering power is 10 mW.
Example 7
The invention is based on NiFe2O4/Ga2O3As shown in fig. 2, the method for manufacturing an ultraviolet photodiode is specifically implemented according to the following steps:
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute, ethylene glycol monomethyl ether (CH)3OCH2CH2OH) as solvent, ethanolamine (HOCH)2CH2NH2) As a stabilizer, the concentration of the solution is 0.6 mol/L;
step 3.2, stirring the solution obtained in the step 1 for two hours at a constant temperature of 60 ℃ to form sol, and filtering the sol after aging for 36 hours;
3.3, spin-coating the sol prepared in the step 2 on the intrinsic SiC homoepitaxial layer, controlling the spin-coating speed to 3000rpm during spin-coating, controlling the spin-coating time to be 30 seconds, carrying out low-temperature heat treatment on a sample obtained after spin-coating at 200 ℃ in an air environment for 20 minutes, and then carrying out high-temperature heat treatment at 600 ℃ for 25 minutes by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the sample is cooled to the room temperature in the air, spin coating and heat treatment are carried out according to the step 3.3, and the repetition times of the spin coating and the heat treatment are adjusted to control the prepared N-type beta-Ga2O3The thickness of the layer is 150 nm;
and 3.5, placing the sample obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 800 ℃, and the annealing time is 2 hours.
Step 4, adopting a magnetron sputtering method to perform P-type NiFe2O4Making electrode on the layer, firstly using Ti as sputtering target material and making it be in P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 4Pa and controlling the sputtering power to be 150W; and then, sputtering Au as a sputtering target material on the surface of the Ti layer to form an Au layer, wherein the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 3Pa, and the sputtering power is 15 mW.
Step 5, adopting a magnetron sputtering method to carry out magnetron sputtering on the N-type beta-Ga2O3Preparing electrodes on the layer, firstly using Ni as target material to make N-type beta-Ga2O3Sputtering the surface of the layer to form a Ni layer, controlling the sputtering time to be 1 hour, controlling the sputtering pressure to be 4 and controlling the sputtering power to be 100; and then, sputtering Au as a sputtering target material on the surface of the Ni layer to form an Au layer, wherein the sputtering time is controlled to be 1 hour, the sputtering pressure is controlled to be 3Pa, and the sputtering power is 15 mW.
Claims (1)
1. Based on NiFe2O4/Ga2O3The preparation method of the ultraviolet photodiode is characterized by comprising the following steps:
step 1, cleaning a substrate (1), and drying the substrate with nitrogen for later use;
the cleaning process in the step 1 comprises the following steps: gradually cleaning the sample by using cleaning solution-acetone-alcohol-deionized water;
step 2, carrying out P-type NiFe on the substrate (1) cleaned in the step 12O4Growing a layer;
p-type NiFe on the substrate (1) in the step 22O4The layer is grown by adopting a magnetron sputtering device and NiFe2O4Ceramic material as target material, argon Ar and oxygen O2As sputtering gas, Ar: O in sputtering2The proportion is 10: 1-5: 1, the substrate temperature is 500-600 ℃, the sputtering pressure is controlled to be 0.5-5 Pa, the sputtering power is controlled to be 100-200W, the sputtering time is controlled to be 0.1-5 hours, then the sample obtained by sputtering is annealed in the air environment, the annealing temperature is 600-700 ℃, the annealing time is 0.5-2 hours, and the P-type NiFe is obtained2O4A heteroepitaxial layer;
step 3, obtaining P type NiFe in step 22O4Carrying out N-type beta-Ga on partial region on the layer2O3Growing a layer;
in the step 3, a sol-gel method is adopted to carry out the preparation of P-type NiFe2O4Growing N-type beta-Ga in layer region2O3Layer of Ga (NO)3)3xH2O as Ga source and ethylene glycol monomethyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As the stabilizer, the following are specific:
step 3.1, preparing a solution: with Ga (NO)3)3xH2O as solute and glycol methyl ether CH3OCH2CH2OH as solvent, ethanolamine HOCH2CH2NH2As a stabilizer, the concentration of the solution is 0.3-0.6 mol/L;
step 3.2, stirring the solution obtained in the step 3.1 at a constant temperature of 60-70 ℃ for 2-3 hours to form sol, and filtering the sol after aging for 36-48 hours;
step 3.3, configuring the step 3.2Sol is coated on P type NiFe by spinning2O4On the layer, the spin coating speed is controlled to be 2500-3000 rpm during spin coating, the spin coating time is controlled to be 30-45 seconds, the material obtained after spin coating is subjected to low-temperature heat treatment for 10-40 minutes in an air environment at the temperature of 100-200 ℃, and then is subjected to high-temperature heat treatment for 10-40 minutes at the temperature of 500-700 ℃ by using a rapid annealing furnace;
step 3.4, after the heating treatment, after the material is cooled to room temperature in the air, carrying out secondary spin coating and heat treatment, and controlling the repetition times of the spin coating and the heat treatment to prepare the N-type beta-Ga2O3The thickness of the layer;
step 3.5, placing the material obtained after the spin coating and the heat treatment in an air environment for annealing treatment, wherein the annealing temperature is 600-1000 ℃, and the annealing time is 1-3 hours to obtain the N-type beta-Ga2O3A layer;
step 4, obtaining P type NiFe in step 22O4Making P-type NiFe on the layer2O4An electrode (3) on the layer;
in the step 4, the P type NiFe2O4The electrode is made by magnetron sputtering, firstly Ti is used as sputtering target material to be sputtered on P-type NiFe2O4Sputtering the surface of the heteroepitaxial layer to form a Ti layer, wherein the sputtering time is controlled to be 0.1-2 hours, the sputtering pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W; then, Au is used as a sputtering target material to sputter on the surface of the Ti layer to form an Au layer, the sputtering time is controlled to be 0.1-2 hours, the sputtering pressure is controlled to be 2-4 Pa, and the sputtering power is 10-20 mW;
step 5, obtaining N-type beta-Ga in step 32O3Layer-by-layer fabrication of N-type beta-Ga2O3An electrode (5) on the layer eventually forming said NiFe-based2O4/Ga2O3The ultraviolet photodiode of (1);
in the step 5, the N-type beta-Ga2O3When electrodes are manufactured on the layers, magnetron sputtering is adopted, firstly, Ni is used as a target material, the deposition time is controlled to be 0.1-2 hours, the deposition pressure is controlled to be 0.1-10 Pa, and the sputtering power is controlled to be 100-200W; then, Au is used as a sputtering target material to sputter on the surface of the Ni layer to form an Au layer, and the deposition time is controlledThe preparation is carried out for 0.1-2 hours, the deposition pressure is controlled to be 2-4 Pa, the sputtering power is 10-20 mW, and the NiFe-based alloy is finally formed2O4/Ga2O3The ultraviolet photodiode of (1);
based on NiFe2O4/Ga2O3The ultraviolet photodiode comprises a substrate (1), wherein P type NiFe is formed on the substrate (1)2O4Layer (2), P-type NiFe2O4N-type beta-Ga is formed on a partial region of the layer (2)2O3Layer (4), N-type beta-Ga2O3The layer (4) is provided with N-type beta-Ga2O3Electrode (5) on the layer, P-type NiFe2O4The other partial region of the layer (2) is formed with P-type NiFe2O4An electrode (3) on the layer, the P type NiFe2O4Electrode (3) on the layer and N-type beta-Ga2O3The electrode (5) on the layer is made of one of Au, Al, Ni, Ti, Cu and Pb metal materials, or alloy or ITO conductive compound containing the metal materials, and the substrate (1) is Al2O3Quartz, insulating MgO or insulating SrTiO3Substrate of said N-type beta-Ga2O3The thickness of the layer (4) is 100-200 nm, and the doping concentration is 1015～1016cm-3Said P type NiFe2O4The layer (2) has a thickness of 100 to 200nm and a carrier concentration of 1017～1018cm-3。
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